ES2346124B2 - PROCESS FOR PURIFICATION OF XYLOOLIGOSACARIDS BASED ON THE USE OF DIAFILTRATION. - Google Patents
PROCESS FOR PURIFICATION OF XYLOOLIGOSACARIDS BASED ON THE USE OF DIAFILTRATION. Download PDFInfo
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- ES2346124B2 ES2346124B2 ES200900117A ES200900117A ES2346124B2 ES 2346124 B2 ES2346124 B2 ES 2346124B2 ES 200900117 A ES200900117 A ES 200900117A ES 200900117 A ES200900117 A ES 200900117A ES 2346124 B2 ES2346124 B2 ES 2346124B2
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- xylooligosaccharides
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- liquors
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- 238000000746 purification Methods 0.000 title claims abstract description 23
- 238000011026 diafiltration Methods 0.000 title claims abstract description 15
- 235000013305 food Nutrition 0.000 claims abstract description 19
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- 238000006731 degradation reaction Methods 0.000 claims abstract description 3
- 238000012545 processing Methods 0.000 claims description 18
- 229920001542 oligosaccharide Polymers 0.000 claims description 16
- 150000002482 oligosaccharides Chemical class 0.000 claims description 15
- 238000001728 nano-filtration Methods 0.000 claims description 14
- 150000004823 xylans Chemical class 0.000 claims description 14
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 240000005979 Hordeum vulgare Species 0.000 description 2
- 235000007340 Hordeum vulgare Nutrition 0.000 description 2
- 239000001888 Peptone Substances 0.000 description 2
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- 150000007513 acids Chemical class 0.000 description 2
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- 125000000089 arabinosyl group Chemical group C1([C@@H](O)[C@H](O)[C@H](O)CO1)* 0.000 description 2
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- 235000005822 corn Nutrition 0.000 description 2
- 238000005115 demineralization Methods 0.000 description 2
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- 238000011036 discontinuous diafiltration Methods 0.000 description 2
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- 238000004108 freeze drying Methods 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
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- 150000002989 phenols Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000006041 probiotic Substances 0.000 description 2
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- 238000011084 recovery Methods 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 150000008163 sugars Chemical class 0.000 description 2
- 239000012138 yeast extract Substances 0.000 description 2
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 1
- 241000186000 Bifidobacterium Species 0.000 description 1
- 241000186018 Bifidobacterium adolescentis Species 0.000 description 1
- 241001608472 Bifidobacterium longum Species 0.000 description 1
- 241000186015 Bifidobacterium longum subsp. infantis Species 0.000 description 1
- 229920001706 Glucuronoxylan Polymers 0.000 description 1
- 241000218657 Picea Species 0.000 description 1
- 241000228182 Thermoascus aurantiacus Species 0.000 description 1
- 229940004120 bifidobacterium infantis Drugs 0.000 description 1
- 229940009291 bifidobacterium longum Drugs 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
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- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 230000008020 evaporation Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 235000021255 galacto-oligosaccharides Nutrition 0.000 description 1
- 150000003271 galactooligosaccharides Chemical class 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
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- 238000010327 methods by industry Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
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- 230000010287 polarization Effects 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 150000004804 polysaccharides Chemical class 0.000 description 1
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- 108090000623 proteins and genes Proteins 0.000 description 1
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- 230000000930 thermomechanical effect Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 125000000969 xylosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)CO1)* 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/06—Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
Proceso para la purificación de xilooligosacáridos.Process for purification of xylooligosaccharides.
La presente invención, titulada "Proceso para la purificación de xilooligosacáridos", reivindica un procedimiento aplicable a la purificación de xilooligosacáridos obtenidos mediante degradación hidrolítica (por vía química y/o enzimática) de la fracción hemicelulósica de biomasa vegetal en medio acuoso. Los licores de hidrólisis contienen xilooligosacáridos junto con otros componentes no deseados, que deben ser eliminados para permitir la utilización de los xilooligosacáridos con fines alimentarios. Este objetivo se consigue por medio de diafiltración (eventualmente, en combinación con otras operaciones de naturaleza físico-química que se describen en el texto de la solicitud). Se reivindica la utilización de las fracciones conteniendo xilooligosacáridos purificados como ingredientes alimentarios con propiedades prebióticas, aplicables en la nutrición humana y en la alimentación animal.The present invention, entitled "Process for the purification of xylooligosaccharides, "claims a procedure applicable to the purification of xylooligosaccharides obtained by hydrolytic degradation (by chemical and / or enzymatic) of the hemicellulosic fraction of plant biomass in aqueous medium. Hydrolysis liquors contain xylooligosaccharides together with other unwanted components, which must be removed to allow the use of xylooligosaccharides for purposes food This objective is achieved through diafiltration. (eventually, in combination with other operations of a nature physicochemical that are described in the text of the request). The use of the fractions is claimed containing purified xylooligosaccharides as ingredients food with prebiotic properties, applicable in nutrition Human and animal feed.
Description
Proceso para la purificación de xilooligosacáridos.Process for purification of xylooligosaccharides.
La invención plantea la aplicación de técnicas básicas de la Química y de la Ingeniería Química (operaciones de concentración y separación) a la purificación de disoluciones obtenidas por procesamiento químico de biomasa vegetal rica en hemicelulosas. Por las aplicaciones alimentarias del producto final y por tratarse del desarrollo de un proceso químico, el objeto de esta patente también está relacionado con áreas de la técnica como la Tecnología de los Alimentos, Ingeniería de los Alimentos e Ingeniería de Procesos.The invention raises the application of techniques Basic Chemistry and Chemical Engineering (operations of concentration and separation) to the purification of solutions obtained by chemical processing of plant biomass rich in hemicelluloses For food applications of the final product and because it is the development of a chemical process, the object of This patent is also related to areas of the art such as Food Technology, Food Engineering and Process engineering.
La biomasa vegetal tiene una estructura heterogénea y una composición variable en función de su origen. Sus componentes incluyen polisacáridos (celulosa, hemicelulosas y pectinas), compuestos fenólicos libres (extraíbles sin reacción química) o ligados (formando parte de macromoléculas), proteínas, componentes inorgánicos y otras fracciones de poca importancia para los fines de esta invención. Algunos tipos de biomasa (como maderas de frondosas, salvados y determinados residuos agrícolas) tienen hemicelulosas principalmente constituidas por xilano (formado por unidades de xilosa unidas por enlaces \beta 1-4), en donde los monómeros estructurales pueden estar sustituidos (por ejemplo, con azúcares, compuestos fenólicos, ácidos urónicos o metil urónicos, y/o grupos acetilo). Información relevante sobre estos puntos aparece publicada en los siguientes trabajos: Ebringerová, A.; Heinze, T., Xylan and xylan derivatives - biopolymers with valuable properties. 1. Naturally occurring xylans: structures, isolation procedures and properties, Macromol. Rapid Commun. 2000, 21, 542-556; y Ebringerová, A.; Hromádková, Z.; Heinze, T., Hemicellulose, Adv. Polym. Sci. 2005, 186, 1-67.Vegetable biomass has a structure Heterogeneous and a variable composition depending on its origin. Their Components include polysaccharides (cellulose, hemicelluloses and pectins), free phenolic compounds (extractable without reaction chemistry) or bound (forming part of macromolecules), proteins, inorganic components and other fractions of little importance to The purposes of this invention. Some types of biomass (such as wood of hardwood, bran and certain agricultural residues) have hemicelluloses mainly constituted by xylan (formed by xylose units linked by β 1-4 bonds), where the structural monomers can be substituted (by example, with sugars, phenolic compounds, uronic acids or methyl uronic, and / or acetyl groups). Relevant information about these points is published in the following works: Ebringerová, TO.; Heinze, T., Xylan and xylan derivatives - biopolymers with valuable properties. 1. Naturally occurring xylans: structures, isolation procedures and properties, Macromol. Rapid Commun 2000, 21, 542-556; and Ebringerová, A .; Hromádková, Z .; Heinze, T., Hemicellulose, Adv. Polym Sci. 2005, 186, 1-67.
La hidrólisis parcial por vía química de las hemicelulosas conteniendo xilano puede conducir a mezclas de composición compleja, formadas por polímeros derivados del xilano de menor peso molecular que el polímero original, xilooligómeros, xilosa, otros monosacáridos, subproductos de reacción de los monosacáridos (por ejemplo, furfural e hidroximetilfurfural), ácido acético, metanol, componentes inorgánicos, compuestos nitrogenados, fracciones extraíbles presentes en la materia prima y otros componentes de menor interés para la finalidad de esta patente. Alternativa o complementariamente, pueden generarse xilooligosacáridos mediante enzimas con actividad xilanásica, que pueden actuar sobre biomasa nativa conteniendo xilano, sobre fracciones de biomasa enriquecidas en xilano por procesamiento químico previo, o sobre disoluciones que procedan del fraccionamiento químico de biomasa en donde aparezcan fracciones poliméricas solubles derivadas del xilano. Información complementaria sobre este tema puede encontrarse en los siguientes artículos: Vázquez, M. J.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Xylooligosaccharides. Manufacture and applications, Trends Food Sci. Technol. 2000, 11, 387-393; y Moure, A.; Gullón, P.; Domínguez, H.; Parajó, J. C., Advances in the manufacture, purification and applications of xylooligosaccharides as food additives and nutraceuticals, Proc. Biochem. 2006, 41, 1913-1923. Más específicamente, se han publicado datos sobre la producción de xilooligosacáridos por la acción directa de xilanasas sobre zuros de maíz (Katapodis, P.; Christakopoulos, P., Enzymic production of feruloyl xylooligosaccharides from corn cobs by a family 10 xylanase from Thermoascus aurantiacus, LWT - Food Sci. Technol. 2008, 41, 1239-1243), por tratamiento directo de materiales lignocelulósicos en medio acuoso (Carvalheiro, F.; Garrote, G.; Parajó, J. C.; Pereira, H.; Girio, F. M., Kinetic modeling of brewery's spent grain autohydrolysis, Biotechnol. Prog. 2005, 21, 233-243; Garrote, G.; Domínguez, H.; Parajó, J. C., Production of substituted oligosaccharides by hydrolytic processing of barley husks, Ind. Eng. Chem. Res. 2004, 43, 1608-1614) y por procesamiento enzimático de licores de autohidrólisis (Vegas, R.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Enzymatic processing of rice husk autohydrolysis products for obtaining low molecular weight oligosaccharides, Food Biotechnol. 2008, 22, 31-46; Vázquez, M. J.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Enzymatic processing of crude xylooligomer solutions obtained by autohydrolysis of Eucalyptus wood, Food Biotechnol. 2002, 16, 91-105).Partial hydrolysis by chemical route of hemicelluloses containing xylan can lead to mixtures of complex composition, formed by polymers derived from xylan of lower molecular weight than the original polymer, xylo-oligomers, xylose, other monosaccharides, reaction by-products of monosaccharides (for example , furfural and hydroxymethylfurfural), acetic acid, methanol, inorganic components, nitrogen compounds, extractable fractions present in the raw material and other components of less interest for the purpose of this patent. Alternatively or in addition, xylooligosaccharides can be generated by enzymes with xylanic activity, which can act on native biomass containing xylan, on biomass fractions enriched in xylan by prior chemical processing, or on solutions that come from chemical biomass fractionation where soluble polymeric fractions appear Xylan derivatives. Additional information on this subject can be found in the following articles: Vázquez, MJ; Alonso, JL; Dominguez, H .; Paradox, JC, Xylooligosaccharides. Manufacture and applications, Trends Food Sci. Technol. 2000, 11, 387-393; and Moure, A .; Gullón, P .; Dominguez, H .; Parajó, JC, Advances in the manufacture, purification and applications of xylooligosaccharides as food additives and nutraceuticals, Proc. Biochem 2006, 41, 1913-1923. More specifically, data on the production of xylooligosaccharides have been published by the direct action of xylanases on corn walls (Katapodis, P .; Christakopoulos, P., Enzymic production of feruloyl xylooligosaccharides from corn cobs by a family 10 xylanase from Thermoascus aurantiacus , LWT - Food Sci. Technol. 2008, 41, 1239-1243), by direct treatment of lignocellulosic materials in aqueous medium (Carvalheiro, F .; Garrote, G .; Parajó, JC; Pereira, H .; Girio, FM, Kinetic modeling of brewery's spent grain autohydrolysis, Biotechnol. Prog. 2005, 21, 233-243; Garrote, G .; Dominguez, H .; Parajó, JC, Production of substituted oligosaccharides by hydrolytic processing of barley husks, Ind. Eng. Chem. Res. 2004, 43, 1608-1614) and by enzymatic processing of autohydrolysis liquors (Vegas, R .; Alonso, JL; Domínguez, H .; Parajó, JC, Enzymatic processing of rice husk autohydrolysis products for obtaining low molecular weight oligosaccharides , Food Biotechnol. 2008, 22, 31-46; Vázquez, MJ; Alonso, JL; Dominguez, H .; Paradox, JC, Enzymatic processing of crude xylooligomer solutions obtained by autohydrolysis of Eucalyptus wood, Food Biotechnol. 2002, 16, 91-105).
Los xilooligosacáridos se obtienen en medios que también contienen otros productos no deseados. Esto es particularmente cierto en los casos donde los xilooligosacáridos se obtienen por métodos basados en el procesamiento químico de biomasa vegetal nativa, donde la composición de los medios puede ser muy compleja. Puede encontrarse información sobre este punto en las siguientes referencias: Garrote, G.; Kabel, M. A.; Schols, H. A.; Falqué, E.; Domínguez, H.; Parajó, J. C., Effects of Eucalyptus globulus wood autohydrolysis conditions on the reaction products. J. Agric. Food Chem. 2007, 55, 9006-9013; y Garrote, G.; Falqué, E.; Domínguez, H.; Parajó, J. C., Autohydrolysis of agricultural residues: study of reaction byproducts, Biores. Technol. 2007, 98, 1951-1957.Xylooligosaccharides are obtained in media that also contain other unwanted products. This is particularly true in cases where xylooligosaccharides are obtained by methods based on the chemical processing of native plant biomass, where the composition of the media can be very complex. Information on this point can be found in the following references: Garrote, G .; Kabel, MA; Schols, HA; Falqué, E .; Dominguez, H .; Paradox, JC, Effects of Eucalyptus globulus wood autohydrolysis conditions on the reaction products. J. Agric. Food Chem. 2007, 55, 9006-9013; and Garrote, G .; Falqué, E .; Dominguez, H .; Parajó, JC, Autohydrolysis of agricultural residues: study of reaction byproducts, Biores. Technol 2007, 98, 1951-1957.
Para obtener xilooligosacáridos de calidad alimentaria se necesita purificar los productos de reacción, aplicando distintos procedimientos físico-químicos, como los que se incluyen en las siguientes referencias: Parajó, J. C.; Domínguez, H.; Alonso, J. L.; Vázquez, M. J.; Garrote, G., Proceso para la purificación de oligosacáridos obtenidos a partir de biomasa, Patente española con número de solicitud P200102313, fecha de solicitud 22.10.2001, fecha de aplicación: 01.07.2003; Vázquez, M. J.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Production and refining of soluble products from Eucalyptus globulus glucuronoxylan, Collect. Czech. Chem. Comm. 2007, 72, 307-320; Vázquez, M. J.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Enhancing the potential of oligosaccharides from corncob autohydrolysis as prebiotic food ingredients, Ind. Crops Prod. 2006, 24, 152-159; Vázquez, M. J.; Garrote, G.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Refining of autohydrolysis liquors for manufacturing xylooligosaccharides: evaluation of operational strategies, Biores. Technol. 2005, 96, 889-896.To obtain food grade xylooligosaccharides, the reaction products need to be purified, applying different physical-chemical procedures, such as those included in the following references: Parajó, JC; Dominguez, H .; Alonso, JL; Vázquez, MJ; Garrote, G., Process for the purification of oligosaccharides obtained from biomass, Spanish patent with application number P200102313, date of application 22.10.2001, date of application: 01.07.2003; Vázquez, MJ; Alonso, JL; Dominguez, H .; Parajó, JC, Production and refining of soluble products from Eucalyptus globulus glucuronoxylan, Collect. Czech Chem. Comm. 2007, 72, 307-320; Vázquez, MJ; Alonso, JL; Dominguez, H .; Parajo, JC, Enhancing the potential of oligosaccharides from corncob autohydrolysis as prebiotic food ingredients, Ind. Crops Prod. 2006, 24, 152-159; Vázquez, MJ; Garrote, G .; Alonso, JL; Dominguez, H .; Parajó, JC, Refining of autohydrolysis liquors for manufacturing xylooligosaccharides: evaluation of operational strategies, Biores. Technol 2005, 96, 889-896.
La bibliografía científica y técnica está prestando una atención creciente a la aplicación de tecnologías de membrana para la generación de xilooligosacáridos (Freixo, M. R.; Norberta de Pinho, M., Enzymatic hydrolysis of beechwood xylan in a membrane reactor, Desalination, 2002, 149, 237-242; González-Muñoz, M. J.; Domínguez, H.; Parajó, J. C., Depolymerization of xylan-derived products in an enzymatic membrane reactor, J. Membr. Sci. 2008, 320, 224-231), para su concentración (Yuan, Q. P.; Zhang, H.; Qian, Z. M.; Yang, X. J., Pilot-plant production of xylo-oligosaccharides from corncob by sleaming, enzymatic hydrolysis and nanofiltration, J. Chem. Technol. Biotechnol. 2004, 79, 1073-1079) o para su purificación (Vegas, R.; Moure, A.; Domínguez, H.; Parajó, J. C.; Álvarez, J. R.; Luque, S., Purification of oligosaccharides from rice husk autohydrolysis liquors by ultra- and nano-filtration, Desalination 2006, 199, 541-543; Vegas, R.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Manufacture and refining of oligosaccharides from industrial solid wastes, Ind. Eng. Chem. Res. 2005, 44, 614-620; Vegas, R.; Luque, S.; Álvarez, J. R.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Membrane-assisted processing of xylooligosaccharide-containing liquors, J. Agric. Food Chem. 2006, 54, 5430-5436; Gullón, P.; González-Muñoz, M. J.; Domínguez, H.; Parajó, J. C., Membrane processing of liquors from Eucalyptus globulus autohydrolysis, J. Food Eng. 2008, 87, 257-265). No se ha encontrado información bibliográfica sobre la purificación de xilooligosacáridos por procesos basados en diafiltración, un modo de operación que presenta ventajas respecto a otras alternativas de procesamiento con membranas, al mejorar la purificación, limitar la polarización por concentración (con el consecuente aumento del flujo de permeado), y disminuir el consumo energético y el gasto de disolvente.The scientific and technical literature is paying increasing attention to the application of membrane technologies for the generation of xylooligosaccharides (Freixo, MR; Norberta de Pinho, M., Enzymatic hydrolysis of beechwood xylan in a membrane reactor, Desalination, 2002, 149, 237-242; González-Muñoz, MJ; Domínguez, H .; Parajó, JC, Depolymerization of xylan-derived products in an enzymatic membrane reactor, J. Membr. Sci. 2008, 320, 224-231), for its concentration ( Yuan, QP; Zhang, H .; Qian, ZM; Yang, XJ, Pilot-plant production of xylo-oligosaccharides from corncob by sleaming, enzymatic hydrolysis and nanofiltration, J. Chem. Technol. Biotechnol. 2004, 79, 1073-1079 ) or for purification (Vegas, R .; Moure, A .; Dominguez, H .; Parajó, JC; Álvarez, JR; Luque, S., Purification of oligosaccharides from rice husk autohydrolysis liquors by ultra- and nano-filtration, Desalination 2006, 199, 541-543; Vegas, R .; Alonso, JL; Domínguez, H .; Parajó, JC, Manufacture and refining of oligosaccharides from industrial solid wastes, Ind. Eng. Chem. Res. 2005, 44, 614-620; Vegas, R .; Luque, S .; Álvarez, JR; Alonso, JL; Dominguez, H .; Parajó, JC, Membrane-assisted processing of xylooligosaccharide-containing liquors, J. Agric. Food Chem. 2006, 54, 5430-5436; Gullón, P .; González-Muñoz, MJ; Dominguez, H .; Paradox, JC, Membrane processing of liquors from Eucalyptus globulus autohydrolysis, J. Food Eng. 2008, 87, 257-265). No bibliographic information was found on the purification of xylooligosaccharides by diafiltration-based processes, a mode of operation that has advantages over other membrane processing alternatives, by improving purification, limiting concentration polarization (with the consequent increase in flow permeate), and decrease energy consumption and solvent expenditure.
La diafiltración es un modo de operación en que se lleva a cabo una ultrafiltración o nanofiltración con aporte de disolvente añadido. El disolvente puede añadirse continuamente con el mismo caudal que el permeado (modo de operación que se conoce como diafiltración a volumen constante), añadirse continuamente con un caudal menor que el del permeado (modo de operación que se conoce como diafiltración a volumen variable), o bien añadirse por lotes a tiempos de operación determinados (modo de operación que se conoce como diafiltración discontinua). Cualquiera de estos modos de operación resulta aplicable a la invención que se reivindica. La bibliografía cita aplicaciones de la diafiltración en los siguientes campos: aislamiento de hemicelulosas (Krawczyk, H.; Persson, T.; Andersson, A.; Jönsson, A. S., Isolation of hemicelluloses from barley husks, Food Bioprod. Proc. 2008, 86, 31-36; Andersson, A.; Persson, T.; Zacchi, G.; Staalbrand, H.; Joensson, A. S., Comparison of diafiltration and size-exclusion chromatography to recover hemicelluloses from process water from thermomechanical pulping of spruce, Appl. Biochem. Biotechnol. 2007, 137-140, 971-983), refinado de medios fermentativos (Wang, L.; Yang, G.; Xing, W.; Xu, N., Mathematic model of the yield for diafiltration processes, Sep. Purif. Technol. 2008, 59, 206-213), separación de polifenoles y azúcares (Wei, D. S.; Hossain, M.; Saleh, Z. S., Separation of polyphenolics and sugar by ultrafiltration: effects of operating conditions on fouling and diafiltration, Int. J. Chem. Biomolec. Eng. 2008, 1, 10-17), desmineralización de permeados de leche y suero (Suárez, E.; Lobo, A.; Álvarez-Blanco, S.; Riera, F. A.; Álvarez, R., Utilization of nanofiltration membranes for whey and milk ultrafiltration permeate demineralization, Desalination 2006, 199, 345-347), recuperación de oligosacáridos a partir de leche (Martinez-Ferez, A.; Guadix, A.; Guadix, E. M., Recovery of caprine milk oligosaccharides with ceramic membranes, J. Membr. Sci. 2006, 276, 23-30), y purificación de mezclas de galactooligosacáridos comerciales (Goulas, A. K.; Kapasakalidis, P. G.; Sinclair, H. R.; Rastall, R. A.; Grandison, A. S., Purification of oligosaccharides by nanofiltration, J. Membr. Sci. 2002, 209, 321-335). Ninguna de estas aplicaciones se solapa con la purificación de xilooligosacáridos contenidos en medios de hidrólisis de biomasa, tema objeto de esta invención.Diafiltration is a mode of operation in which ultrafiltration or nanofiltration is carried out with the contribution of solvent added. The solvent can be added continuously with the same flow rate as the permeate (operating mode known as constant volume diafiltration), be added continuously with a lower flow rate than permeate (known mode of operation as variable volume diafiltration), or be added in batches to set operating times (operating mode known as discontinuous diafiltration). Any of these modes of operation is applicable to the claimed invention. The bibliography cites diafiltration applications in the following fields: hemicellulose isolation (Krawczyk, H .; Persson, T .; Andersson, A .; Jönsson, A. S., Isolation of hemicelluloses from Barley Husks, Food Bioprod. Proc. 2008, 86, 31-36; Andersson, A .; Persson, T .; Zacchi, G .; Staalbrand, H .; Joensson, A. S., Comparison of diafiltration and size-exclusion chromatography to recover hemicelluloses from process water from thermomechanical pulping of spruce, Appl. Biochem Biotechnol 2007, 137-140, 971-983), refined from fermentative media (Wang, L .; Yang, G .; Xing, W .; Xu, N., Mathematic model of the yield for diafiltration processes, Sep. Purif. Technol 2008, 59, 206-213), separation of polyphenols and sugars (Wei, D. S .; Hossain, M .; Saleh, Z. S., Separation of polyphenolics and sugar by ultrafiltration: effects of operating conditions on fouling and diafiltration, Int. J. Chem. Biomolec Eng. 2008, 1, 10-17), demineralization of milk and whey permeate (Suárez, E .; Lobo, A .; Álvarez-Blanco, S .; Riera, F. A .; Álvarez, R., Utilization of nanofiltration membranes for whey and milk ultrafiltration permeate demineralization, Desalination 2006, 199, 345-347), recovery of oligosaccharides from milk (Martinez-Ferez, A .; Guadix, A .; Guadix, E. M., Recovery of caprine milk oligosaccharides with ceramic membranes, J. Membr. Sci. 2006, 276, 23-30), and purification of commercial galactooligosaccharide mixtures (Goulas, A. K .; Kapasakalidis, P. G .; Sinclair, H. R .; Rastall, R. TO.; Grandison, A. S., Purification of oligosaccharides by nanofiltration, J. Membr. Sci. 2002, 209, 321-335). None of these applications overlap with the purification of xylooligosaccharides contained in biomass hydrolysis media, Subject of this invention.
Cabe destacar que, una vez purificados, los xilooligosacáridos tienen carácter de moléculas bioactivas, con poder prebiótico y con otras propiedades biológicas que dependen de su naturaleza química (particularmente, del grado de sustitución, tipo de sustituyentes y distribución de pesos moleculares). Puede encontrase información sobre estos temas en las referencias Vázquez, M. J.; Alonso, J. L.; Domínguez, H.; Parajó, J. C., Xylooligosaccharides. Manufacture and applications, Trends Food Sci. Technol. 2000, 11, 387-393; y Moure, A.; Gullón, P.; Domínguez, H.; Parajó, J. C., Advances in the manufacture, purification and applications of xylooligosaccharides as food additives and nutraceuticals, Proc. Biochem. 2006, 41,1913-1923.It should be noted that, once purified, the Xylooligosaccharides have the character of bioactive molecules, with prebiotic power and with other biological properties that depend on its chemical nature (particularly, of the degree of substitution, type of substituents and molecular weight distribution). May information on these topics can be found in the Vázquez references, M. J .; Alonso, J. L .; Dominguez, H .; Parajó, J. C., Xylooligosaccharides. Manufacture and applications, Trends Food Sci. Technol 2000, 11, 387-393; and Moure, A .; Gullón, P .; Dominguez, H .; Parajó, J. C., Advances in the manufacture, purification and applications of xylooligosaccharides as food additives and nutraceuticals, Proc. Biochem 2006, 41,1913-1923.
En base a lo anterior, resulta de interés un proceso de purificación de disoluciones en donde los xilooligosacáridos estuviesen en presencia de compuestos no deseados, y que deberían ser eliminados para permitir la aplicación de los mencionados xilooligosacáridos para fines alimentarios. Para ello, la presente invención se centra en un proceso formado por tratamientos físico-químicos, en los que la diafiltración juega un papel fundamental para conseguir un grado de pureza que permita desarrollar aplicaciones en el ámbito alimentario.Based on the above, it is of interest to solution purification process where xylooligosaccharides were in the presence of compounds not desired, and that should be removed to allow application of the aforementioned xylooligosaccharides for food purposes. For Therefore, the present invention focuses on a process formed by physical-chemical treatments, in which the diafiltration plays a fundamental role in achieving a degree of purity that allows developing applications in the field food
El proceso considerado consiste en someter a los licores de degradación hidrolítica de hemicelulosas de materiales lignocelulósicos ricos en xilano a una secuencia de etapas de purificación, según el Proceso 1 o el Proceso 2 que se describen a continuación.The process considered consists in submitting Hydrolytic degradation liquors of hemicellulose materials Xylan-rich lignocellulosics to a sequence of stages of purification, according to Process 1 or Process 2 described in continuation.
El Proceso 1, destinado principalmente a la purificación de medios conteniendo xilooligosacáridos, de modo que se obtengan productos de bajo peso molecular, consta de:Process 1, intended primarily for purification of media containing xylooligosaccharides, so that low molecular weight products are obtained, consists of:
- a) to)
- una o varias etapas de concentración (opcionales, llevadas a cabo por evaporación a vacío, evaporación rotatoria, ultrafiltración operando en modo concentración o nanofiltración operando en modo concentración, de modo que se obtenga una disolución concentrada en xilooligosacáridos),one or several concentration stages (optional, carried out by vacuum evaporation, rotary evaporation, ultrafiltration operating in concentration or nanofiltration mode operating in concentration mode, so that a concentrated solution in xylooligosaccharides),
- b) b)
- una o varias etapas de diafiltración de los licores originales o de los concentrados obtenidos en el apartado a), para eliminar componentes no deseados de bajo peso molecular,one or several stages of diafiltration of liquors originals or concentrates obtained in section a), for remove unwanted components of low molecular weight,
- c) C)
- procesamiento de los licores diafiltrados obtenidos en el apartado b) en una o varias etapas (opcionales) de ultrafiltración o nanofiltración, operando en modo concentración, de modo que se obtenga una disolución concentrada en xilooligosacáridos,processing of diafiltered liquors obtained in section b) in one or several (optional) stages of ultrafiltration or nanofiltration, operating in concentration mode, of so that a solution concentrated in xylooligosaccharides,
- d) d)
- una etapa de tratamiento de los medios concentrados obtenidos en las condiciones de los apartados b) ó c) con enzimas que presenten actividad xilanásica, a fin de reducir el grado de polimerización de los xilooligosacáridos,a stage of treatment of concentrated media obtained under the conditions of sections b) or c) with enzymes that present xilanase activity, in order to reduce the degree of polymerization of xylooligosaccharides,
- e) and)
- procesamiento del medio de reacción obtenido en las condiciones del apartado d) mediante una o varias etapas de ultrafiltración, nanofiltración o diafiltración, de modo que se obtenga una disolución concentrada en xilooligosacáridos,processing of the reaction medium obtained in the conditions of section d) through one or several stages of ultrafiltration, nanofiltration or diafiltration, so that obtain a solution concentrated in xylooligosaccharides,
- f) F)
- tratamiento (opcional) de las disoluciones refinadas obtenidas en el apartado e) con adsorbentes y/o resinas de cambio iónico, en una o varias etapas, para eliminar compuestos no-sacáridos presentes en el medio,(optional) treatment of refined solutions obtained in section e) with adsorbents and / or exchange resins ionic, in one or several stages, to remove compounds non-saccharides present in the medium,
- g) g)
- deshidratación de las disoluciones obtenidas en el apartado f) por tecnologías convencionales, como la evaporación a vacío, la liofilización o la atomización, para obtener producto sólido purificado conteniendo xilooligosacáridos.dehydration of the solutions obtained in the section f) by conventional technologies, such as evaporation to vacuum, lyophilization or atomization, to obtain product purified solid containing xylooligosaccharides.
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El Proceso 2, destinado principalmente a la purificación de medios conteniendo xilooligosacáridos de alto grado de polimerización, consta de:Process 2, intended primarily for purification of media containing high grade xylooligosaccharides polymerization, consists of:
- a) to)
- una o varias etapas de concentración (opcionales, llevadas a cabo por evaporación a vacío, evaporación rotatoria, ultrafiltración operando en modo concentración o nanofiltración operando en modo concentración, de manera que se obtenga una disolución concentrada en xilooligosacáridos); haciéndose notar que si se emplean ultrafiltración o nanofiltración para fines de concentración, la membrana debe poseer un tamaño molecular de corte suficientemente pequeño para limitar las pérdidas de xilooligosacáridos en el permeado,one or several concentration stages (optional, carried out by vacuum evaporation, rotary evaporation, ultrafiltration operating in concentration or nanofiltration mode operating in concentration mode, so that a concentrated solution in xylooligosaccharides); noting that if ultrafiltration or nanofiltration is used for the purpose of concentration, the membrane must have a molecular size of cut small enough to limit losses of xylooligosaccharides in the permeate,
- b) b)
- tratamiento de los medios originales o de los licores concentrados que surgen del procesamiento indicado en el apartado a) por diafiltración a volumen constante, a volumen variable o discontinua, empleando membranas con un tamaño de corte adecuado para permitir el paso a su través de impurezas de bajo peso molecular, reteniendo los oligosacáridos con grados de polimerización por encima de un valor definido,treatment of the original media or of the concentrated liquors arising from the processing indicated in the section a) by diafiltration at constant volume, at volume variable or discontinuous, using membranes with a cut size suitable to allow passage through impurities of low weight molecular, retaining oligosaccharides with degrees of polymerization above a defined value,
- c) C)
- procesamiento de los licores retenidos operando en las condiciones del apartado b) en una o varias etapas (opcionales) de ultrafiltración o nanofiltración, operando en modo concentración, de modo que se obtenga una disolución concentrada en xilooligosacáridos,processing of retained liquors operating in the conditions of section b) in one or several stages (optional) ultrafiltration or nanofiltration, operating in concentration mode, so that a solution concentrated in xylooligosaccharides,
- d) d)
- tratamiento (opcional) del retenido obtenido en los apartados b) ó c) con adsorbentes y/o resinas de cambio iónico, en una o varias etapas, para eliminar compuestos no-sacáridos presentes en el medio,treatment (optional) of the retained obtained in the sections b) or c) with adsorbents and / or ion exchange resins, in one or several stages, to eliminate compounds non-saccharides present in the medium,
- e) and)
- la deshidratación de las disoluciones obtenidas en los apartados b), c) ó d) por tecnologías convencionales, como la evaporación a vacío, la liofilización o la atomización, para obtener un producto sólido purificado conteniendo xilooligosacáridos.dehydration of the solutions obtained in Sections b), c) or d) by conventional technologies, such as vacuum evaporation, lyophilization or atomization, to obtain a purified solid product containing xylooligosaccharides.
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Un posible modo de realización del Proceso 1 se describe a continuación en el Ejemplo 1.A possible way of carrying out Process 1 is described below in Example 1.
Se parte de licores del procesamiento acuoso de cáscaras de arroz, obtenidos en las condiciones de operación recomendadas en el artículo siguiente: González-Muñoz, M. J.; Domínguez, H.; Parajó, J. C., Depolymerization of xylan-derived products in an enzymatic membrane reactor, J. Membr. Sci. 2008, 320, 224-231, con la salvedad de que el procesamiento hidrotérmico se realizó isotérmicamente a 185ºC durante 20 minutos. La composición de los licores se midió empleando los métodos descritos en la misma referencia, llegándose a los siguientes resultados de concentración (medidos como gramos de componente por cada 100 g de solutos no volátiles): glucosa 0.68, xilosa 2.92, arabinosa 3.53, ácido acético 3.80, glucooligosacáridos (medidos como glucosa) 9.03, xilooligosacáridos (medidos como xilosa) 43.1, sustituyentes arabinosil (medidos como arabinosa) 2.35, sustituyentes acetilo (medidos como ácido acético) 2.90, sustituyentes urónicos (medidos como ácido galacturónico) 4.26, otros componentes no volátiles 31.25. Empleando agua como disolvente añadido, los licores se sometieron a diafiltración continua, hasta llegar a una relación de 1 volumen de disolvente añadido/volumen inicial. La composición del concentrado resultante se midió empleando los métodos a los que se aludió anteriormente, llegándose a los siguientes resultados de concentración (medidos como gramos de componente por cada 100 g de solutos no volátiles): glucosa 0.39, xilosa 1.38, arabinosa 1.63, ácido acético 1.70, glucooligosacáridos (medidos como glucosa) 11.2, xilooligosacáridos (medidos como xilosa) 48.2, sustituyentes arabinosil (medidos como arabinosa) 2.65, sustituyentes acetilo (medidos como ácido acético) 3.57, sustituyentes urónicos (medidos como ácido galacturónico) 4.93, otros componentes no volátiles 26.04. Esta disolución se concentró empleando una membrana de nanofiltración hasta obtener una relación volumen final/volumen inicial de 5, obteniéndose un concentrado con la siguiente composición: glucosa 0.20, xilosa 0.42, arabinosa 0.43, ácido acético 0.41, glucooligosacáridos (medidos como glucosa) 13.1, xilooligosacáridos (medidos como xilosa) 53.8, sustituyentes arabinosil (medidos como arabinosa) 3.34, sustituyentes acetilo (medidos como ácido acético) 4.20, sustituyentes urónicos (medidos como ácido galacturónico) 5.21, otros componentes no volátiles 19.34. Esta disolución se empleó para llevar a cabo una etapa de hidrólisis enzimática con xilanasas comerciales (manteniendo una actividad de 685 Unidades Internacionales/kg licor en medio a pH 7), que se prolongó durante 48 horas a 55ºC. El medio de reacción se sometió a ultrafiltración operando en modo concentración, obteniéndose un permeado con las siguientes concentraciones (medidas como gramos de componente por cada 100 g de solutos no volátiles): glucosa 1.06, xilosa 0.79, arabinosa 0.70, ácido acético 1.27, glucooligosacáridos (medidos como glucosa) 13.2, xilooligosacáridos (medidos como xilosa) 60.9, sustituyentes arabinosil (medidos como arabinosa) 3.34, sustituyentes acetilo (medidos como ácido acético) 4.33, sustituyentes urónicos (medidos como ácido galacturónico) 4.88, otros componentes no volátiles 10.8. Esta disolución se puso en contacto con la resina comercial IRA-96 (cambiadora de aniones), operando con una relación másica de 15 g licor/g resina, obteniéndose una disolución con la siguiente composición (medida como gramos de componente por cada 100 g de solutos no volátiles): glucosa 1.07, xilosa 0.60, arabinosa 0.81, ácido acético 2.16, glucooligosacáridos (medidos como glucosa) 14.6; xilooligosacáridos (medidos como xilosa) 68.2; sustituyentes arabinosil (medidos como arabinosa) 2.88; sustituyentes acetilo (medidos como ácido acético) 3.85, sustituyentes urónicos (medidos como ácido galacturónico) 4.85, otros componentes no volátiles 3.16. La disolución resultante se liofilizó, obteniéndose un polvo blanco-amarillento. Puede observarse que la suma de xilooligosacáridos y sus sustituyentes (grupos arabinosil, grupos acetilo, grupos urónicos) ha aumentado su proporción respecto al total de solutos no volátiles desde un 59.4% en los licores crudos de autohidrólisis hasta un 79.8% en el producto final. Si se considera también la presencia de glucooligosacáridos, que potencialmente pueden tener propiedades prebióticas, la proporción de oligosacáridos totales (glucooligosacáridos y xilooligosacáridos sustituidos) respecto al total de solutos no volátiles aumenta desde un 70.6% en los licores crudos de autohidrólisis hasta el 94.4% en el producto final. Estos datos ponen de manifiesto los efectos de purificación obtenidos con el proceso que se reivindica, y que suponen la eliminación selectiva de monosacáridos y de otros componentes no deseados. A fin de confirmar el carácter prebiótico de los productos purificados obtenidos en el Ejemplo 2, éstos se emplearon como fuente de carbono para el cultivo de las mismas cepas de bacterias probióticas citadas en el Ejemplo 1, elaborándose medios de cultivo en condiciones de anaerobiosis que contenían 5 g/L de extracto de levadura, 5 g/L de peptona y 10 g/L del producto liofilizado obtenido en el Ejemplo 2. Se tomaron alícuotas de este medio, que se depositaron en tubos de cultivo herméticos antes de su esterilización en autoclave. Posteriormente, se inocularon con las bacterias anteriormente citadas y se incubaron a 37ºC sin agitación. Al cabo de 12 y 24 horas se realizaron recuentos de células al microscopio, que confirmaron la susceptibilidad de las fuentes de carbono empleadas para el crecimiento celular. En una serie de experimentos adicional, se llevaron a cabo fermentaciones utilizando las mismas condiciones de cultivo que las descritas en el párrafo anterior, pero empleando como inoculo heces humanas. Al cabo de 96 horas de incubación se procedió al análisis de las muestras por Cromatografía Líquida de Alta Eficacia (según el procedimiento citado con anterioridad), confirmándose el consumo completo de oligosacáridos.Be part of liquors from the aqueous processing of rice husks, obtained under operating conditions Recommended in the following article: González-Muñoz, M. J .; Dominguez, H .; Paradox, J. C., Depolymerization of xylan-derived products in an enzymatic membrane reactor, J. Membr. Sci. 2008, 320, 224-231, with the proviso that the processing Hydrothermal was performed isothermally at 185 ° C for 20 minutes. The composition of the liquors was measured using the methods described in the same reference, reaching the following concentration results (measured as grams of component per per 100 g of nonvolatile solutes): glucose 0.68, xylose 2.92, arabinose 3.53, acetic acid 3.80, glucooligosaccharides (measured as glucose) 9.03, xylooligosaccharides (measured as xylose) 43.1, arabinosyl substituents (measured as arabinose) 2.35, acetyl substituents (measured as acetic acid) 2.90, uronic substituents (measured as galacturonic acid) 4.26, other nonvolatile components 31.25. Using water as solvent added, the liquors underwent continuous diafiltration, until reach a ratio of 1 volume of solvent added / volume initial. The composition of the resulting concentrate was measured using the methods referred to above, reaching to the following concentration results (measured as grams of component per 100 g of nonvolatile solutes): glucose 0.39, xylose 1.38, arabinose 1.63, acetic acid 1.70, glucooligosaccharides (measured as glucose) 11.2, xylooligosaccharides (measured as xylose) 48.2, arabinosyl substituents (measured as arabinose) 2.65, acetyl substituents (measured as acetic acid) 3.57, uronic substituents (measured as galacturonic acid) 4.93, other non-volatile components 26.04. This solution was concentrated. using a nanofiltration membrane until obtaining a relationship final volume / initial volume of 5, obtaining a concentrate with The following composition: glucose 0.20, xylose 0.42, arabinose 0.43, acetic acid 0.41, glucooligosaccharides (measured as glucose) 13.1, xylooligosaccharides (measured as xylose) 53.8, substituents arabinosyl (measured as arabinose) 3.34, acetyl substituents (measured as acetic acid) 4.20, uronic substituents (measured as galacturonic acid) 5.21, other non-volatile components 19.34. This solution was used to carry out a stage of Enzymatic hydrolysis with commercial xylanases (maintaining a activity of 685 International Units / kg liquor in medium at pH 7), which lasted for 48 hours at 55 ° C. The reaction medium is underwent ultrafiltration operating in concentration mode, obtaining a permeate with the following concentrations (measured as grams of component per 100 g of nonvolatile solutes): glucose 1.06, xylose 0.79, arabinose 0.70, acetic acid 1.27, glucooligosaccharides (measured as glucose) 13.2, xylooligosaccharides (measured as xylose) 60.9, arabinosyl substituents (measured as arabinose) 3.34, acetyl substituents (measured as acetic acid) 4.33, uronic substituents (measured as galacturonic acid) 4.88, other nonvolatile components 10.8. This solution was put in contact with the commercial resin IRA-96 (anion exchanger), operating with a mass ratio of 15 g liquor / g resin, obtaining a solution with the following composition (measured as grams of component per 100 g of nonvolatile solutes): glucose 1.07, xylose 0.60, arabinose 0.81, acetic acid 2.16, glucooligosaccharides (measured as glucose) 14.6; xylooligosaccharides (measured as xylose) 68.2; substituents arabinosyl (measured as arabinose) 2.88; acetyl substituents (measured as acetic acid) 3.85, uronic substituents (measured as galacturonic acid) 4.85, other nonvolatile components 3.16. The resulting solution was lyophilized, obtaining a powder yellowish white. It can be seen that the sum of xylooligosaccharides and their substituents (arabinosyl groups, groups acetyl, uronic groups) has increased its proportion with respect to Total non-volatile solutes from 59.4% in raw liquors of autohydrolysis up to 79.8% in the final product. Whether also considers the presence of glucooligosaccharides, which they can potentially have prebiotic properties, the proportion of total oligosaccharides (glucooligosaccharides and xylooligosaccharides replaced) with respect to total non-volatile solutes increases from 70.6% in raw autohydrolysis liquors up to 94.4% in the final product These data show the effects of purification obtained with the process that is claimed, and that involve the selective elimination of monosaccharides and others unwanted components. In order to confirm the prebiotic character of the purified products obtained in Example 2, these are used as a source of carbon for the cultivation of the same strains of probiotic bacteria cited in Example 1, elaborating culture media under anaerobic conditions containing 5 g / L of yeast extract, 5 g / L of peptone and 10 g / L of the product lyophilisate obtained in Example 2. Aliquots of this were taken medium, which were deposited in airtight culture tubes before their autoclave sterilization. Subsequently, they were inoculated with the bacteria mentioned above and incubated at 37 ° C without shaking. After 12 and 24 hours, cell counts were performed at microscope, which confirmed the susceptibility of the sources of carbon used for cell growth. In a series of additional experiments, fermentations were carried out using the same culture conditions as described in the paragraph previous, but using human feces as inoculum. After 96 incubation hours the samples were analyzed by High Efficiency Liquid Chromatography (according to the procedure cited above), confirming the full consumption of oligosaccharides
Un posible modo de realización del Proceso 2 se describe a continuación en el Ejemplo 2.A possible way of carrying out Process 2 is described below in Example 2.
\vskip1.000000\baselineskip\ vskip1.000000 \ baselineskip
Se parte de licores del procesamiento acuoso de madera de eucalipto, obtenidos en las condiciones de operación recomendadas en el artículo siguiente: Gullón, P.; González-Muñoz, M. J.; Domínguez, H.; Parajó, J. C.; Membrane processing of liquors from Eucalyptus globulus autohydrolysis, J. Food Eng. 2008, 87, 257-265; con la salvedad de que se realizó un pretratamiento acuoso a 130ºC para eliminar extractos, y que la temperatura máxima del tratamiento hidrolítico de las hemicelulosas se fijó en 175ºC. La composición de los licores se midió empleando los métodos descritos en la misma referencia, llegándose a los siguientes resultados de concentración (medidos como gramos de componente por cada 100 g de solutos no volátiles): glucosa 0.31, xilosa 5.29, arabinosa 2.04, ácido acético 1.82, glucooligosacáridos (medidos como glucosa) 1.71, xilooligosacáridos (medidos como xilosa) 53.1, sustituyentes acetilo (medidos como ácido acético) 12.5, sustituyentes urónicos (medidos como ácido galacturónico) 16.5, otros componentes no volátiles 8.55. Empleando agua como disolvente añadido, los licores se sometieron a diafiltración discontinua en 3 etapas sucesivas, en que se alcanzaron relaciones de volúmenes de concentración de 1.67, 1.67 y 3.35 volúmenes de retenido/volumen inicial, respectivamente. La composición del concentrado resultante se midió empleando los métodos a los que se aludió anteriormente, llegándose a los siguientes resultados de concentración (medidos como gramos de componente por cada 100 g de solutos no volátiles): glucosa 0.04, xilosa 1.29, arabinosa 0.44, ácido acético 0.31, glucooligosacáridos (medidos como glucosa) 2.52, xilooligosacáridos (medidos como xilosa) 67.4, sustituyentes acetilo (medidos como ácido acético) 14.5, ácidos urónicos y otros componentes no volátiles, 12.99). A continuación, se realizó una etapa de adsorción con la resina comercial IRA-96 (cambiadora de aniones), operando con una relación másica de 7.5 g licor/g resina. La composición de la disolución (medida como gramos de componente por cada 100 g de solutos no volátiles) fue la siguiente: glucosa 0.002, xilosa 1.89, arabinosa 0.65, ácido acético 0.21, glucooligosacáridos (medidos como glucosa) 4.43, xilooligosacáridos (medidos como xilosa) 67.4, sustituyentes acetilo (medidos como ácido acético) 14.5, sustituyentes urónicos (medidos como ácido galacturónico) 7.45, otros componentes no volátiles 3.7. Puede observarse que la suma de xilooligosacáridos y sus sustituyentes (grupos arabinosil, grupos acetilo, grupos urónicos) ha aumentado su proporción respecto al total de solutos no volátiles desde 82.1% en los licores crudos de autohidrólisis hasta 89.6% en los productos finales. Si se considera también la presencia de glucooligosacáridos, que potencialmente pueden tener propiedades prebióticas, la proporción de oligosacáridos totales (glucooligosacáridos y xilooligosacáridos sustituidos) respecto al total de solutos no volátiles aumenta desde un 83.8% en los licores crudos de autohidrólisis hasta un 94%. Estos datos ponen de manifiesto los efectos de purificación obtenidos con el proceso que se reivindica, y que suponen la eliminación selectiva de monosacáridos y de otros componentes no deseados. A fin de confirmar el carácter prebiótico de los productos purificados, éstos se emplearon como fuente de carbono para el cultivo de cepas de bacterias probióticas (Bifidobacterium adolescentis CECT 5781, equivalente a ATCC 15703; Bifidobacterium longum CECT 4503, equivalente a ATCC 15707; Bifidobacterium infantis CECT 4551, equivalente a ATCC 15697; y Bifidobacterium breve CECT 4839, correspondiente a ATCC 15700). Todas las cepas se obtuvieron de la Colección Española de Cultivos Tipo (CECT, Valencia, España). En condiciones de anaerobiosis, se elaboraron medios de cultivo conteniendo 5 g/L de extracto de levadura, 5 g/L de peptona y 10 g/L del producto liofilizado obtenido en el proceso. Se tomaron alícuotas de este medio, que se depositaron en tubos de cultivo herméticos antes de su esterilización en autoclave. Posteriormente, se inocularon con las bacterias anteriormente citadas y se incubaron a 37ºC sin agitación. Al cabo de 12 y 24 horas se realizaron recuentos de células al microscopio, que confirmaron la susceptibilidad de las fuentes de carbono empleadas para el crecimiento celular. En una nueva serie de experimentos, se llevaron a cabo fermentaciones utilizando las mismas condiciones de cultivo que las descritas anteriormente, pero empleando como inoculo heces humanas. Al cabo de 96 horas de incubación se procedió al análisis de las muestras por Cromatografía Líquida de Alta Eficacia (según el procedimiento citado con anterioridad) lo que reveló el consumo completo de oligosacáridos.It is based on liquors from the aqueous processing of eucalyptus wood, obtained under the operating conditions recommended in the following article: Gullón, P .; González-Muñoz, MJ; Dominguez, H .; He stopped, JC; Membrane processing of liquors from Eucalyptus globulus autohydrolysis, J. Food Eng. 2008, 87, 257-265; with the proviso that an aqueous pretreatment was carried out at 130 ° C to remove extracts, and that the maximum temperature of the hydrolytic treatment of hemicelluloses was set at 175 ° C. The composition of the liquors was measured using the methods described in the same reference, reaching the following concentration results (measured as grams of component per 100 g of nonvolatile solutes): glucose 0.31, xylose 5.29, arabinose 2.04, acetic acid 1.82, glucooligosaccharides (measured as glucose) 1.71, xylooligosaccharides (measured as xylose) 53.1, acetyl substituents (measured as acetic acid) 12.5, uronic substituents (measured as galacturonic acid) 16.5, other nonvolatile components 8.55. Using water as an added solvent, the liquors were subjected to discontinuous diafiltration in 3 successive stages, in which ratios of concentration volumes of 1.67, 1.67 and 3.35 retention volumes / initial volume, respectively, were reached. The composition of the resulting concentrate was measured using the methods mentioned above, reaching the following concentration results (measured as grams of component per 100 g of nonvolatile solutes): glucose 0.04, xylose 1.29, arabinose 0.44, acid acetic 0.31, glucooligosaccharides (measured as glucose) 2.52, xylooligosaccharides (measured as xylose) 67.4, acetyl substituents (measured as acetic acid) 14.5, uronic acids and other nonvolatile components, 12.99). Next, an adsorption stage was carried out with the commercial resin IRA-96 (anion exchanger), operating with a mass ratio of 7.5 g liquor / g resin. The composition of the solution (measured as grams of component per 100 g of non-volatile solutes) was as follows: glucose 0.002, xylose 1.89, arabinose 0.65, acetic acid 0.21, glucooligosaccharides (measured as glucose) 4.43, xylooligosaccharides (measured as xylose ) 67.4, acetyl substituents (measured as acetic acid) 14.5, uronic substituents (measured as galacturonic acid) 7.45, other non-volatile components 3.7. It can be seen that the sum of xylooligosaccharides and their substituents (arabinosyl groups, acetyl groups, uronic groups) has increased its proportion with respect to total non-volatile solutes from 82.1% in raw autohydrolysis liquors to 89.6% in final products. If the presence of glucooligosaccharides, which can potentially have prebiotic properties, is also considered, the proportion of total oligosaccharides (glucooligosaccharides and substituted xylooligosaccharides) with respect to total non-volatile solutes increases from 83.8% in raw autohydrolysis liquors to 94%. These data show the purification effects obtained with the claimed process, and that involve the selective elimination of monosaccharides and other unwanted components. In order to confirm the prebiotic nature of the purified products, these were used as a carbon source for the cultivation of strains of probiotic bacteria ( Bifidobacterium adolescentis CECT 5781, equivalent to ATCC 15703; Bifidobacterium longum CECT 4503, equivalent to ATCC 15707; Bifidobacterium infantis CECT 4551, equivalent to ATCC 15697; and Bifidobacterium brief CECT 4839, corresponding to ATCC 15700). All strains were obtained from the Spanish Type Culture Collection (CECT, Valencia, Spain). Under anaerobic conditions, culture media were prepared containing 5 g / L of yeast extract, 5 g / L of peptone and 10 g / L of the lyophilized product obtained in the process. Aliquots of this medium were taken, which were deposited in airtight culture tubes before autoclaving. Subsequently, they were inoculated with the aforementioned bacteria and incubated at 37 ° C without shaking. After 12 and 24 hours, cell counts were performed under a microscope, which confirmed the susceptibility of the carbon sources used for cell growth. In a new series of experiments, fermentations were carried out using the same culture conditions as described above, but using human feces as inoculum. After 96 hours of incubation, the samples were analyzed by High Efficiency Liquid Chromatography (according to the procedure mentioned above) which revealed the complete consumption of oligosaccharides.
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| Title |
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| GOULAS, A.K., et al. Purification of oligosaccharides by nanofiltration. Journal of Membrane Science. 2002. N$^{o}$ 209, pp. 321-335. Ver Abstract, Introduction y pp. 331 (punto 4.3). * |
| GULLÓN, P. et al. Membrane processing of liquors from Eucalyptus globulus autohydrolysis. Journal of Food Engineering, 2008. N$^{o}$ 87, pp. 257-265. Ver Abstrac e Introduction. * |
| NABARLATZ, D. et al. Purification of xylooligosaccharides from almond shells by ultrafiltrationSeparation and Purification Technology. 2007, n$^{o}$ 53, pp. 235-243. Ver Abstract y Conclusions. * |
| VÁZQUEZ, M.J. et al. Enzymatic processing of crude xylooligomer solution obtained by autohydrolysis of eucaliptus wood. 2002. Vol. 16, n$^{o}$ 2, pp. 91-105. Ver Abstract e Introduction. * |
| VEGAS, R. et al. Evaluation of nanofiltration for refining soluble products fron rice husk xylan. Bioresource Technology. 2008. N$^{o}$ 99, pp. 5341-5351. Ver abstract e Introduction. * |
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